US20220344083A1 - R-t-b series permanent magnet material, raw material composition preparation method and application - Google Patents
R-t-b series permanent magnet material, raw material composition preparation method and application Download PDFInfo
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Images
Classifications
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- H—ELECTRICITY
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- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T428/12014—All metal or with adjacent metals having metal particles
Definitions
- the present disclosure relates to an R-T-B series permanent magnet material, a raw material composition, a preparation method, and an application.
- Permanent magnet materials have been developed as key materials to support electronic devices, and the development is in the direction of high magnetic energy product and high coercivity.
- R-T-B series permanent magnet materials (where R is at least one of the rare earth elements) are known as magnets with the highest performance among permanent magnets, and are used in various motors and home appliances such as voice coil motors (VCM) for hard disk drives, motors for electric vehicles (EV, HV, PHV etc.), and motors for industrial equipment.
- VCM voice coil motors
- EV electric vehicles
- HV electric vehicles
- PHV etc. motors for industrial equipment.
- R 6 -T 13 -X a high amount of one or more of Cu, Al and Ga is added thereto to generate R 6 -T 13 -X (X refers to Cu, Al and/or Ga) in order to improve the performance; however, R 6 -T 13 -X is relatively sensitive to heat treatment temperature and time (as described in WO 2013008756 and WO 0124203), and during bulk treatment in a large heat treatment furnace, the performance of the permanent magnet material varies greatly depending on the loading position, which is not conducive to mass production.
- the technical problem to be solved by the present disclosure is to provide an R-T-B series permanent magnet material, a raw material composition, a preparation method, and an application thereof, in order to overcome the deficiency in existing R-T-B series permanent magnet materials that when the content of B is less than 5.88 at %, the generation of R 6 -T 13 -X in order to improve magnetic performance results in a magnet being sensitive to heat treatment temperature and time, which is not conducive to mass production of an R-T-B series permanent magnet material with an excellent magnetic performance.
- R-T-B series permanent magnet material comprising, by mass percentage, the following components:
- wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material; the R-T-B series permanent magnet material further comprises Co and Ti; N includes Cu and/or Ga; R includes RL and RH, wherein RL is a light rare earth element, including at least Nd, and RH is a heavy rare earth element; an (RL 1-y RH y ) 2 Ti 7 C x phase is present at the grain boundary of the R-T-B series permanent magnet material, wherein x is 2-3, y is 0.15-0.35, and T necessarily includes Fe, and also includes one or more of Co, Ti and N.
- the type of RH may include one or more of Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, and Sc.
- the type of RL may include one or more of La, Ce, Pr, Pm, Sm, and Eu.
- the grain boundary of the R-T-B series permanent magnet material refers to the position between adjacent two or more main phase crystal grains.
- the R-T-B series permanent magnet material may further comprise M, and M includes one or more of the elements Al, Si, Sn, Ge, Ag, Au, Bi, Mn, Cr, Zr, Nb, and Hf.
- the range of the content of M is preferably 0-3 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- the range of the content of Cu is preferably 0.05-0.20 wt. %, e.g. 0.12 wt. %, 0.08 wt. % or 0.15 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- the range of the content of Ga is preferably 0.05-0.20 wt. %, e.g. 0.12 wt. %, 0.12 wt. % or 0.1 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- the R-T-B series permanent magnet material may further comprise 0, and the range of the content of 0 may be 0.08-0.12 wt. %, e.g. 0.09 or 0.1 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- x in the (RL 1-y RH y ) 2 Ti 7 C x phase, x may be 2-2.8, e.g. 2.6 or 2.7. y may be 0.15-0.3, e.g. 0.18, 0.22, 0.23 or 0.28.
- the (RL 1-y RH y ) 2 T 17 C x phase is (RL 0.77 RH 0.23 ) 2 -T 17 -C 2.7 , (RL 0.78 RH 0.22 ) 2 -T 17 -C 2.6 , (RL 0.77 RH 0.23 ) 2 -T 17 -C 2.8 , (RL 0.81 RH 0.18 ) 2 -T 17 -C 2.7 , or (RL 0.72 RH 0.28 ) 2 -T 17 -C 2.8 .
- the range of the content of R is 30.2-31.0 wt. % or 29-30.4 wt. %, e.g. 30 wt. %, 30.4 wt. % or 31 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- the type of RH includes Dy and/or Tb.
- the range of the content of RH is 1-2.5 wt. %, exclusive of 1 wt. %, e.g. 1.9 wt. %, 2 wt. % or 1.5 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- the range of the content of B is 0.905-0.93 wt. %, e.g. 0.93 wt. %, 0.905 wt. % or 0.915 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- the range of the content of C is 0.1-0.15 wt. % or 0.04-0.12 wt. %, e.g. 0.12 wt. %, 0.07 wt. % or 0.1 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- the content of Ti may be a conventional amount in the art.
- the range of the content of Ti is 0.05-0.2 wt. % or 0.1-0.25 wt. %, e.g. 0.16 wt. %, 0.08 wt. % or 0.1 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- the content of Co may be a conventional amount in the art.
- the range of the content of Co is 0.5-1.5 wt. % or 1-2 wt. %, e.g. 0.8 wt. %, 1.2 wt. %, 1 wt. % or 1.5 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 30.2-31.0 wt. % of R, 1-2.5 wt. % of RH, 0.905-0.93 wt. % of B, 0.1-0.15 wt. % of C, 0.05-0.2 wt. % of Ti, 0.5-1.5 wt. % of Co, and 0.08-0.12 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 29-30.4 wt. % of R, 1-2.5 wt. % of RH, 0.905-0.93 wt. % of B, 0.04-0.12 wt. % of C, 0.1-0.25 wt. % of Ti, 1-2 wt. % of Co, and 0.08-0.12 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 28.5 wt. % of Nd, 0.6 wt. % of Dy, 1.3 wt. % of Tb, 0.93 wt. % of B, 0.12 wt. % of C, 0.12 wt. % of Cu, 0.12 wt. % of Ga, 0.16 wt. % of Ti, 0.8 wt. % of Co, and 0.08 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 29 wt. % of PrNd, 1.5 wt. % of Dy, 0.5 wt. % of Tb, 0.905 wt. % of B, 0.04 wt. % of C, 0.2 wt. % of Cu, 0.2 wt. % of Ga, 0.08 wt. % of Ti, 1.2 wt. % of Co, and 0.09 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 27.5 wt. % of Nd, 1 wt. % of Dy, 0.5 wt. % of Tb, 0.945 wt. % of B, 0.15 wt. % of C, 0.05 wt. % of Cu, 0.12 wt. % of Ga, 0.05 wt. % of Ti, 1 wt. % of Co, and 0.1 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 29.5 wt. % of PrNd, 1 wt. % of Dy, 0.5 wt. % of Tb, 0.905 wt. % of B, 0.07 wt. % of C, 0.08 wt. % of Cu, 0.1 wt. % of Ga, 0.1 wt. % of Ti, 1.5 wt. % of Co, and 0.12 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 28.5 wt. % of Nd, 1 wt. % of Dy, 0.5 wt. % of Tb, 0.915 wt. % of B, 0.1 wt. % of C, 0.15 wt. % of Cu, 0.05 wt. % of Ga, 0.2 wt. % of Ti, 2 wt. % of Co, and 0.1 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the present disclosure further provides a raw material composition for an R-T-B series permanent magnet material, comprising, by mass percentage, the following components:
- wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material; wherein the raw material composition for the R-T-B series permanent magnet material comprises Ti and Co; N includes Cu and/or Ga; R includes RL and RH, wherein RL is a rare earth element, including at least Nd, and RH is a heavy rare earth element.
- the range of the content of Cu is preferably 0.05-0.20 wt. %, e.g. 0.12 wt. %, 0.08 wt. % or 0.15 wt. %, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material.
- the range of the content of Ga is preferably 0.05-0.20 wt. %, e.g. 0.12 wt. %, 0.12 wt. % or 0.1 wt. %, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material.
- the type of RH includes Dy and/or Tb.
- the range of the content of RH is 0.5-2 wt. %, exclusive of 0.5 wt. %, e.g. 1.4 wt. %, 1.5 wt. % or 1 wt. %, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material.
- the range of the content of Ti is 0.05-0.2 wt. % or 0.1-0.25 wt. %, e.g. 0.16 wt. %, 0.08 wt. % or 0.1 wt. %, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material.
- the range of the content of Co is 0.5-1.5 wt. % or 1-2 wt. %, e.g. 0.8 wt. %, 1.2 wt. %, 1 wt. % or 1.5 wt. %, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material.
- the raw material composition for the R-T-B series permanent magnet material comprises the following components: 29.7-30.5 wt. % of R, 0.5-2 wt. % of RH, 0.905-0.93 wt. % of B, 0.1-0.15 wt. % of C, 0.05-0.2 wt. % of Ti, and 0.5-1.5 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the raw material composition for the R-T-B series permanent magnet material comprises the following components: 28.5-29.9 wt. % of R, 0.5-2 wt. % of RH, 0.905-0.93 wt. % of B, 0.04-0.12 wt. % of C, 0.1-0.25 wt. % of Ti, and 1-2 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the raw material composition for the R-T-B series permanent magnet material comprises the following components: 28.5 wt. % of Nd, 0.1 wt. % of Dy, 1.3 wt. % of Tb, 0.93 wt. % of B, 0.12 wt. % of C, 0.12 wt. % of Cu, 0.12 wt. % of Ga, 0.16 wt. % of Ti, and 0.8 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the raw material composition for the R-T-B series permanent magnet material comprises the following components: 29 wt. % of PrNd, 1.5 wt. % of Dy, 0.905 wt. % of B, 0.04 wt. % of C, 0.2 wt. % of Cu, 0.2 wt. % of Ga, 0.08 wt. % of Ti, and 1.2 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the raw material composition for the R-T-B series permanent magnet material comprises the following components: 27.5 wt. % of Nd, 0.5 wt. % of Dy, 0.5 wt. % of Tb, 0.945 wt. % of B, 0.15 wt. % of C, 0.05 wt. % of Cu, 0.12 wt. % of Ga, 0.05 wt. % of Ti, and 1 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the raw material composition for the R-T-B series permanent magnet material comprises the following components: 29.5 wt. % of PrNd, 0.5 wt. % of Dy, 0.5 wt. % of Tb, 0.905 wt. % of B, 0.07 wt. % of C, 0.08 wt. % of Cu, 0.1 wt. % of Ga, 0.1 wt. % of Ti, and 1.5 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- the present disclosure further provides a method for preparing an R-T-B series permanent magnet material, comprising the following step: subjecting a melt of the raw material composition for the R-T-B series permanent magnet material to casting, crushing, pulverization, forming, sintering, a grain boundary diffusion treatment, and a heat treatment.
- the melt of the raw material composition for the R-T-B series permanent magnet material can be prepared by means of a conventional method in the art, e.g. by smelting in a high-frequency vacuum induction smelting furnace.
- the degree of vacuum in the smelting furnace may be 5 ⁇ 10 ⁇ 2 Pa.
- the smelting temperature may be 1500° C. or less.
- the casting process may be a conventional casting process in the art, e.g. cooling at a rate of 10 2 to 10 4 ° C./sec in an Ar atmosphere, e.g. in an Ar atmosphere of 5.5 ⁇ 10 4 Pa.
- the dehydrogenation may be carried out under the condition of evacuation while heating.
- the pulverization process may be a conventional pulverization process in the art, e.g. jet mill pulverization.
- the oxidizing gas refers to oxygen or moisture content.
- the pressure in a pulverization chamber for the jet mill pulverization may be 0.38 MPa.
- the time for the jet mill pulverization may be 3 hours.
- a lubricant such as zinc stearate
- the lubricant may be added in an amount of 0.05-0.15%, e.g. 0.12%, 0.06%, 0.15% or 0.08%, relative to the weight of the pulverized powder.
- the content of C in the R-T-B series permanent magnet material may be adjusted by adjusting the added amount of zinc stearate.
- the forming process may be a conventional forming process in the art, e.g. a magnetic field forming method or a hot pressing thermal deformation method.
- the sintering process may be a conventional sintering process in the art, e.g. preheating, sintering, and cooling under vacuum condition, e.g. in a vacuum of 5 ⁇ 10 ⁇ 3 Pa.
- the preheating temperature may be 300-600° C.
- the preheating time may be 1-2 h.
- the preheating is carried out at 300° C. and 600° C., each for 1 h.
- the sintering temperature may be a conventional sintering temperature in the art, e.g. 900-1100° C., further 1040° C.
- the temperature of the grain boundary diffusion treatment may be 800-900° C., e.g. 850° C.
- the time for the grain boundary diffusion treatment may be 12-48 h, e.g. 24 h.
- the present disclosure further provides the use of the R-T-B series permanent magnet material as an electronic component.
- the reagents and raw materials used in the present disclosure are all commercially available.
- the R-T-B series permanent magnet material of the present application has an excellent performance, maintains relatively high Br and Hcj at various heat treatment temperatures: Br ⁇ 13.92 kGs and Hcj ⁇ 25.7 kOe; 2) the R-T-B series permanent magnet material of the present application has wider heat treatment temperature ranges, all with an interval of 40° C. (470-510° C., 460-500° C., and 480-520° C.).
- FIG. 1 is an FE-EPMA surface distribution diagram of the element Nd in the R-T-B series permanent magnet material prepared in Example 1, wherein point 1 is (RL 0.77 RH 0.23 ) 2 -T 17 -C 2.7 .
- Micro-pulverization process The powder pulverized by hydrogen decrepitation was subjected to jet mill pulverization for 3 hours under the conditions of an oxidizing gas content of 100 ppm or less in a nitrogen atmosphere and a pulverization chamber pressure of 0.38 MPa to obtain a fine powder.
- the oxidizing gas referred to oxygen or moisture.
- Zinc stearate was added to the powder resulting from jet mill pulverization in an amount as shown in Table 2, and then fully mixed by means of a V-type mixer.
- Magnetic field forming process The above-mentioned powder, to which zinc stearate had been added, was subjected to primary formation into a cube with a side length of 25 mm by means of a right-angle alignment magnetic field forming machine in a 1.6 T alignment magnetic field at a forming pressure of 0.35 ton/cm 2 , and after the primary formation, the powder was demagnetized in a 0.2 T magnetic field.
- the formed body resulting from primary formation was sealed so that it did not come into contact with air, and secondary formation was then carried out at a pressure of 1.3 ton/cm 2 by means of a secondary formation machine (an isostatic pressing machine).
- compositions of the R-T-B series permanent magnet materials were measured using a high-frequency inductively coupled plasma optical emission spectrometer (ICP-OES), wherein an (RL 1-y RH y ) 2 Ti 7 C x (x: 2-3, and y: 0.15-0.35) phase was obtained according to an FE-EPMA test. Table 3 below showed the composition test results.
- Example 1 30.4 / 28.5 0.6 1.3 0.93 0.12 0.12 0.12 0.16 67.27 / / 0.8 0.08 Yes
- Example 2 31 29 / 1.5 0.5 0.905 0.04 0.2 0.2 0.08 66.29 / / 1.2 0.09 Yes
- Example 3 29 / 27.5 1 0.5 0.945 0.15 0.05 0.12 0.05 68.59 / / 1 0.1 Yes
- Example 4 31 29.5 / 1 0.5 0.905 0.07 0.08 0.1 0.1 66.13 / / 1.5 0.12 Yes
- Example 5 30 / 28.5 1 0.5 0.915 0.1 0.15 0.05 0.2 66.49 / / 2 0.1 Yes Comparative 31.5 30 / 1 0.5 0.96 0.07 0.08 0.07 0.1 66.14 / / 1 0.08 Yes
- Example 1 Comparative 30.6 29.1 / 1 0.5 0.89 0.07 0.04 0.03 0.1 67.19 / / 1 0.08 No Example 2 Comparative 30.9 29.4
- FE-EPMA detection A vertical alignment plane of the permanent magnet material was polished, and detected by means of a field emission-electron probe micro-analyser (FE-EPMA) (JEOL, 8530F). Surface scanning was firstly performed, and phases with different contrasts were then quantitatively analyzed to determine the phase composition, wherein the test conditions were an accelerating voltage of 15 kV and a probe beam current of 50 nA.
- the R-T-B series permanent magnet material of the present application has an excellent performance, maintains relatively high Br and Hcj at various heat treatment temperatures: Br ⁇ 13.92 kGs and Hcj ⁇ 25.7 kOe (Examples 1-5); 2) based on the formula of the present application, even if the contents of R, B, Cu, and Ga are adjusted, no (RL 1-y RH y ) 2 T 17 C x (x: 2-3, and y: 0.15-0.35) phase can be generated, the Br and Hcj of the R-T-B series permanent magnet material cannot be both maintained at higher values, and the heat treatment temperature range is reduced significantly (Comparative Example 1 and Comparative Example 3); 3) based on the formula of the present application, even if the contents of C, Ti and Ga are adjusted, the Hcj of the R-T-B series permanent magnet material is reduced and at the same time the heat treatment temperature range will also decrease when the contents of the other compositions are not within the ranges defined in the present application (Comparative Example 4
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Abstract
Description
- The present disclosure relates to an R-T-B series permanent magnet material, a raw material composition, a preparation method, and an application.
- Permanent magnet materials have been developed as key materials to support electronic devices, and the development is in the direction of high magnetic energy product and high coercivity. R-T-B series permanent magnet materials (where R is at least one of the rare earth elements) are known as magnets with the highest performance among permanent magnets, and are used in various motors and home appliances such as voice coil motors (VCM) for hard disk drives, motors for electric vehicles (EV, HV, PHV etc.), and motors for industrial equipment.
- In order to improve the remanence (abbreviated as Br) of an R-T-B series permanent magnet material, it is usually necessary to reduce the content of B; however, when the content of B is less than 5.88 at %, it can be seen from an Nd—Fe—B ternary phase diagram that R2T17 is easily formed, which R2T17 does not have room temperature uniaxial anisotropy, leading to reduced magnet performance. In the prior art, a high amount of one or more of Cu, Al and Ga is added thereto to generate R6-T13-X (X refers to Cu, Al and/or Ga) in order to improve the performance; however, R6-T13-X is relatively sensitive to heat treatment temperature and time (as described in WO 2013008756 and WO 0124203), and during bulk treatment in a large heat treatment furnace, the performance of the permanent magnet material varies greatly depending on the loading position, which is not conducive to mass production.
- Therefore, there is an urgent need for an R-T-B series permanent magnet material that has not only a guaranteed magnetic performance but also facilitates mass production.
- The technical problem to be solved by the present disclosure is to provide an R-T-B series permanent magnet material, a raw material composition, a preparation method, and an application thereof, in order to overcome the deficiency in existing R-T-B series permanent magnet materials that when the content of B is less than 5.88 at %, the generation of R6-T13-X in order to improve magnetic performance results in a magnet being sensitive to heat treatment temperature and time, which is not conducive to mass production of an R-T-B series permanent magnet material with an excellent magnetic performance.
- The present disclosure provides an R-T-B series permanent magnet material, comprising, by mass percentage, the following components:
- greater than 1 wt. % of RH,
- wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material;
the R-T-B series permanent magnet material further comprises Co and Ti;
N includes Cu and/or Ga;
R includes RL and RH, wherein RL is a light rare earth element, including at least Nd, and RH is a heavy rare earth element;
an (RL1-yRHy)2Ti7Cx phase is present at the grain boundary of the R-T-B series permanent magnet material, wherein x is 2-3, y is 0.15-0.35, and T necessarily includes Fe, and also includes one or more of Co, Ti and N. - In the present disclosure, the type of RH may include one or more of Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, and Sc.
- In the present disclosure, the type of RL may include one or more of La, Ce, Pr, Pm, Sm, and Eu.
- In the present disclosure, the grain boundary of the R-T-B series permanent magnet material refers to the position between adjacent two or more main phase crystal grains.
- In the present disclosure, the R-T-B series permanent magnet material may further comprise M, and M includes one or more of the elements Al, Si, Sn, Ge, Ag, Au, Bi, Mn, Cr, Zr, Nb, and Hf.
- Among them, the range of the content of M is preferably 0-3 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- In the present disclosure, when N includes Cu, the range of the content of Cu is preferably 0.05-0.20 wt. %, e.g. 0.12 wt. %, 0.08 wt. % or 0.15 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- In the present disclosure, when N includes Ga, the range of the content of Ga is preferably 0.05-0.20 wt. %, e.g. 0.12 wt. %, 0.12 wt. % or 0.1 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- In the present disclosure, the R-T-B series permanent magnet material may further comprise 0, and the range of the content of 0 may be 0.08-0.12 wt. %, e.g. 0.09 or 0.1 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- In the present disclosure, in the (RL1-yRHy)2Ti7Cx phase, x may be 2-2.8, e.g. 2.6 or 2.7. y may be 0.15-0.3, e.g. 0.18, 0.22, 0.23 or 0.28. For example, the (RL1-yRHy)2T17Cx phase is (RL0.77RH0.23)2-T17-C2.7, (RL0.78RH0.22)2-T17-C2.6, (RL0.77RH0.23)2-T17-C2.8, (RL0.81RH0.18)2-T17-C2.7, or (RL0.72RH0.28)2-T17-C2.8.
- In the present disclosure, preferably, the range of the content of R is 30.2-31.0 wt. % or 29-30.4 wt. %, e.g. 30 wt. %, 30.4 wt. % or 31 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- In the present disclosure, preferably, the type of RH includes Dy and/or Tb.
- In the present disclosure, preferably, the range of the content of RH is 1-2.5 wt. %, exclusive of 1 wt. %, e.g. 1.9 wt. %, 2 wt. % or 1.5 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- In the present disclosure, preferably, the range of the content of B is 0.905-0.93 wt. %, e.g. 0.93 wt. %, 0.905 wt. % or 0.915 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- In the present disclosure, preferably, the range of the content of C is 0.1-0.15 wt. % or 0.04-0.12 wt. %, e.g. 0.12 wt. %, 0.07 wt. % or 0.1 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- In the present disclosure, the content of Ti may be a conventional amount in the art. Preferably, the range of the content of Ti is 0.05-0.2 wt. % or 0.1-0.25 wt. %, e.g. 0.16 wt. %, 0.08 wt. % or 0.1 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- In the present disclosure, the content of Co may be a conventional amount in the art. Preferably, the range of the content of Co is 0.5-1.5 wt. % or 1-2 wt. %, e.g. 0.8 wt. %, 1.2 wt. %, 1 wt. % or 1.5 wt. %, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material.
- In a preferred embodiment of the present disclosure, the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 30.2-31.0 wt. % of R, 1-2.5 wt. % of RH, 0.905-0.93 wt. % of B, 0.1-0.15 wt. % of C, 0.05-0.2 wt. % of Ti, 0.5-1.5 wt. % of Co, and 0.08-0.12 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- In a preferred embodiment of the present disclosure, the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 29-30.4 wt. % of R, 1-2.5 wt. % of RH, 0.905-0.93 wt. % of B, 0.04-0.12 wt. % of C, 0.1-0.25 wt. % of Ti, 1-2 wt. % of Co, and 0.08-0.12 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- In a preferred embodiment of the present disclosure, the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 28.5 wt. % of Nd, 0.6 wt. % of Dy, 1.3 wt. % of Tb, 0.93 wt. % of B, 0.12 wt. % of C, 0.12 wt. % of Cu, 0.12 wt. % of Ga, 0.16 wt. % of Ti, 0.8 wt. % of Co, and 0.08 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- In a preferred embodiment of the present disclosure, the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 29 wt. % of PrNd, 1.5 wt. % of Dy, 0.5 wt. % of Tb, 0.905 wt. % of B, 0.04 wt. % of C, 0.2 wt. % of Cu, 0.2 wt. % of Ga, 0.08 wt. % of Ti, 1.2 wt. % of Co, and 0.09 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- In a preferred embodiment of the present disclosure, the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 27.5 wt. % of Nd, 1 wt. % of Dy, 0.5 wt. % of Tb, 0.945 wt. % of B, 0.15 wt. % of C, 0.05 wt. % of Cu, 0.12 wt. % of Ga, 0.05 wt. % of Ti, 1 wt. % of Co, and 0.1 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- In a preferred embodiment of the present disclosure, the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 29.5 wt. % of PrNd, 1 wt. % of Dy, 0.5 wt. % of Tb, 0.905 wt. % of B, 0.07 wt. % of C, 0.08 wt. % of Cu, 0.1 wt. % of Ga, 0.1 wt. % of Ti, 1.5 wt. % of Co, and 0.12 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- In a preferred embodiment of the present disclosure, the R-T-B series permanent magnet material comprises, by mass percentage, the following components: 28.5 wt. % of Nd, 1 wt. % of Dy, 0.5 wt. % of Tb, 0.915 wt. % of B, 0.1 wt. % of C, 0.15 wt. % of Cu, 0.05 wt. % of Ga, 0.2 wt. % of Ti, 2 wt. % of Co, and 0.1 wt. % of O, wherein wt. % refers to the mass percentage relative to the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- The present disclosure further provides a raw material composition for an R-T-B series permanent magnet material, comprising, by mass percentage, the following components:
- wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material;
wherein the raw material composition for the R-T-B series permanent magnet material comprises Ti and Co;
N includes Cu and/or Ga;
R includes RL and RH, wherein RL is a rare earth element, including at least Nd, and RH is a heavy rare earth element. - In the present disclosure, when N includes Cu, the range of the content of Cu is preferably 0.05-0.20 wt. %, e.g. 0.12 wt. %, 0.08 wt. % or 0.15 wt. %, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material.
- In the present disclosure, when N includes Ga, the range of the content of Ga is preferably 0.05-0.20 wt. %, e.g. 0.12 wt. %, 0.12 wt. % or 0.1 wt. %, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material.
- In the present disclosure, preferably, the range of the content of R is 29.7-30.5 wt. % or 28.5-29.9 wt. %, e.g. 29.5 wt. %, 29.9 wt. % or 30.5 wt. %, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material.
- In the present disclosure, preferably, the type of RH includes Dy and/or Tb.
- In the present disclosure, preferably, the range of the content of RH is 0.5-2 wt. %, exclusive of 0.5 wt. %, e.g. 1.4 wt. %, 1.5 wt. % or 1 wt. %, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material.
- In the present disclosure, preferably, the range of the content of B is 0.905-0.93 wt. %, e.g. 0.93 wt. %, 0.905 wt. % or 0.915 wt. %, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material.
- In the present disclosure, preferably, the range of the content of Ti is 0.05-0.2 wt. % or 0.1-0.25 wt. %, e.g. 0.16 wt. %, 0.08 wt. % or 0.1 wt. %, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material.
- In the present disclosure, preferably, the range of the content of Co is 0.5-1.5 wt. % or 1-2 wt. %, e.g. 0.8 wt. %, 1.2 wt. %, 1 wt. % or 1.5 wt. %, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material.
- In a preferred embodiment of the present disclosure, the raw material composition for the R-T-B series permanent magnet material, by mass percentage, comprises the following components: 29.7-30.5 wt. % of R, 0.5-2 wt. % of RH, 0.905-0.93 wt. % of B, 0.1-0.15 wt. % of C, 0.05-0.2 wt. % of Ti, and 0.5-1.5 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- In a preferred embodiment of the present disclosure, the raw material composition for the R-T-B series permanent magnet material, by mass percentage, comprises the following components: 28.5-29.9 wt. % of R, 0.5-2 wt. % of RH, 0.905-0.93 wt. % of B, 0.04-0.12 wt. % of C, 0.1-0.25 wt. % of Ti, and 1-2 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- In a preferred embodiment of the present disclosure, the raw material composition for the R-T-B series permanent magnet material, by mass percentage, comprises the following components: 28.5 wt. % of Nd, 0.1 wt. % of Dy, 1.3 wt. % of Tb, 0.93 wt. % of B, 0.12 wt. % of C, 0.12 wt. % of Cu, 0.12 wt. % of Ga, 0.16 wt. % of Ti, and 0.8 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- In a preferred embodiment of the present disclosure, the raw material composition for the R-T-B series permanent magnet material, by mass percentage, comprises the following components: 29 wt. % of PrNd, 1.5 wt. % of Dy, 0.905 wt. % of B, 0.04 wt. % of C, 0.2 wt. % of Cu, 0.2 wt. % of Ga, 0.08 wt. % of Ti, and 1.2 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- In a preferred embodiment of the present disclosure, the raw material composition for the R-T-B series permanent magnet material, by mass percentage, comprises the following components: 27.5 wt. % of Nd, 0.5 wt. % of Dy, 0.5 wt. % of Tb, 0.945 wt. % of B, 0.15 wt. % of C, 0.05 wt. % of Cu, 0.12 wt. % of Ga, 0.05 wt. % of Ti, and 1 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- In a preferred embodiment of the present disclosure, the raw material composition for the R-T-B series permanent magnet material, by mass percentage, comprises the following components: 29.5 wt. % of PrNd, 0.5 wt. % of Dy, 0.5 wt. % of Tb, 0.905 wt. % of B, 0.07 wt. % of C, 0.08 wt. % of Cu, 0.1 wt. % of Ga, 0.1 wt. % of Ti, and 1.5 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- In a preferred embodiment of the present disclosure, the raw material composition for the R-T-B series permanent magnet material, by mass percentage, comprises the following components: 28.5 wt. % of Nd, 0.5 wt. % of Dy, 0.5 wt. % of Tb, 0.915 wt. % of B, 0.1 wt. % of C, 0.15 wt. % of Cu, 0.05 wt. % of Ga, 0.2 wt. % of Ti, and 2 wt. % of Co, wherein wt. % refers to the mass percentage relative to the raw material composition for the R-T-B series permanent magnet material, and the balance is Fe and inevitable impurities.
- The present disclosure further provides a method for preparing an R-T-B series permanent magnet material, comprising the following step: subjecting a melt of the raw material composition for the R-T-B series permanent magnet material to casting, crushing, pulverization, forming, sintering, a grain boundary diffusion treatment, and a heat treatment.
- In the present disclosure, the melt of the raw material composition for the R-T-B series permanent magnet material can be prepared by means of a conventional method in the art, e.g. by smelting in a high-frequency vacuum induction smelting furnace. The degree of vacuum in the smelting furnace may be 5×10−2 Pa. The smelting temperature may be 1500° C. or less.
- In the present disclosure, the casting process may be a conventional casting process in the art, e.g. cooling at a rate of 102 to 104° C./sec in an Ar atmosphere, e.g. in an Ar atmosphere of 5.5×104 Pa.
- In the present disclosure, the crushing process may be a conventional crushing process in the art, e.g. hydrogen absorption, dehydrogenation, and cooling treatment.
- The hydrogen absorption may be carried out under the condition of a hydrogen pressure of 0.15 MPa.
- The dehydrogenation may be carried out under the condition of evacuation while heating.
- In the present disclosure, the pulverization process may be a conventional pulverization process in the art, e.g. jet mill pulverization.
- Preferably, the pulverization process is carried out in an atmosphere with an oxidizing gas content of 100 ppm or less. The oxygen content in the pulverization process is controlled according to a conventional low-oxygen process in the art.
- The oxidizing gas refers to oxygen or moisture content.
- The pressure in a pulverization chamber for the jet mill pulverization may be 0.38 MPa.
- The time for the jet mill pulverization may be 3 hours.
- After pulverization, a lubricant, such as zinc stearate, may be added by a conventional means in the art. The lubricant may be added in an amount of 0.05-0.15%, e.g. 0.12%, 0.06%, 0.15% or 0.08%, relative to the weight of the pulverized powder.
- During the pulverization process, the content of C in the R-T-B series permanent magnet material may be adjusted by adjusting the added amount of zinc stearate.
- In the present disclosure, the forming process may be a conventional forming process in the art, e.g. a magnetic field forming method or a hot pressing thermal deformation method.
- In the present disclosure, the sintering process may be a conventional sintering process in the art, e.g. preheating, sintering, and cooling under vacuum condition, e.g. in a vacuum of 5×10−3 Pa.
- The preheating temperature may be 300-600° C. The preheating time may be 1-2 h. Preferably, the preheating is carried out at 300° C. and 600° C., each for 1 h.
- The sintering temperature may be a conventional sintering temperature in the art, e.g. 900-1100° C., further 1040° C.
- The sintering time may be a conventional sintering time in the art, e.g. 2 h.
- Before cooling, Ar gas may be introduced to make the gas pressure reach 0.1 MPa.
- In the present disclosure, the heavy rare earth element in the grain boundary diffusion treatment includes Dy and/or Tb.
- In the present disclosure, the grain boundary diffusion treatment may be carried out according to a conventional process in the art, e.g. Dy vapor diffusion.
- The temperature of the grain boundary diffusion treatment may be 800-900° C., e.g. 850° C.
- The time for the grain boundary diffusion treatment may be 12-48 h, e.g. 24 h.
- After the grain boundary diffusion treatment, a heat treatment may be further carried out. The heat treatment temperature may be 470-510° C., 460-500° C., or 480-520° C. The time for the heat treatment may be 3 h.
- The present disclosure further provides an R-T-B series permanent magnet material prepared by the above-mentioned preparation method.
- The present disclosure further provides the use of the R-T-B series permanent magnet material as an electronic component.
- On basis of conforming to common knowledge in the art, the above-mentioned preferred conditions can be arbitrarily combined to obtain various preferred embodiments of the present disclosure.
- The reagents and raw materials used in the present disclosure are all commercially available.
- The positive progressive effects of the present disclosure lie in:
- 1) the R-T-B series permanent magnet material of the present application has an excellent performance, maintains relatively high Br and Hcj at various heat treatment temperatures: Br≥13.92 kGs and Hcj≥25.7 kOe;
2) the R-T-B series permanent magnet material of the present application has wider heat treatment temperature ranges, all with an interval of 40° C. (470-510° C., 460-500° C., and 480-520° C.). -
FIG. 1 is an FE-EPMA surface distribution diagram of the element Nd in the R-T-B series permanent magnet material prepared in Example 1, whereinpoint 1 is (RL0.77RH0.23)2-T17-C2.7. - The present disclosure is further described below by way of examples; however, the present disclosure is not limited to the scope of the described examples. For the experimental methods in which no specific conditions are specified in the following examples, selections are made according to conventional methods and conditions or according to the product instructions.
-
TABLE 1 Formula of raw material composition for R-T-B series permanent magnet material and contents (wt. %) RL RH No. R PrNd Nd Dy Tb B Cu Ga Ti Fe Zr Nb Co Example 1 29.8 / 28.5 0 1.3 0.93 0.12 0.12 0.16 68.07 / / 0.8 Example 2 30.5 29 / 1.5 0 0.905 0.2 0.2 0.08 66.92 / / 1.2 Example 3 28.5 / 27.5 1 0 0.945 0.05 0.12 0.05 69.34 / / 1 Example 4 30.5 29.5 / 1 0 0.905 0.08 0.1 0.1 66.82 / / 1.5 Example 5 29.5 / 28.5 1 0 0.915 0.15 0.05 0.2 67.19 / / 2 Comparative 31 30 / 1 0 0.96 0.08 0.07 0.1 66.79 / / 1 Example 1 Comparative 30.1 29.1 / 1 0 0.89 0.04 0.03 0.1 67.84 / / 1 Example 2 Comparative 30.4 29.4 / 1 0 0.97 0.25 0.3 0.1 66.98 / / 1 Example 3 Comparative 29 / 28 1 0 0.945 0.05 0.25 0.02 68.74 / / 1 Example 4 Comparative 28.5 / 27.5 1 0 0.945 0.05 0.12 0.05 69.35 / / 1 Example 5 Comparative 30.5 29 / 1.5 0 0.905 0.2 0.2 / 67.12 0.08 / 1 Example 6 Comparative 30.5 29 / 1.5 0 0.905 0.2 0.2 / 67.12 / 0.08 1 Example 7 Note: “/” refers to being free of the element. -
TABLE 2 Process conditions for Examples 1-5 and Comparative Examples 1-7 Does grain Grain boundary Heat Zinc boundary diffused treatment stearate diffusion heavy rare temperature No. (%) occur? earth element (° C.) Example 1 0.12% Yes Dy 470-510 Example 2 0.06% Yes Tb 460-500 Example 3 0.15% Yes Tb 480-520 Example 4 0.08% Yes Tb 480-520 Example 5 0.08% Yes Tb 460-500 Comparative 0.08% Yes Tb 480-500 Example 1 Comparative 0.08% Yes Tb 460-470 Example 2 Comparative 0.08% Yes Tb 480-500 Example 3 Comparative 0.2% Yes Tb 480-490 Example 4 Comparative 0.16% No / 480-490 Example 5 Comparative 0.06% Yes Tb 480-500 Example 6 Comparative 0.06% Yes Tb 480-500 Example 7 Note: % with regard to zinc stearate refers to the mass percentage in the powder after mixing; “/” refers to being free of the element. - (1) Smelting process: According to the formula shown in Table 1 and the corresponding process conditions in Table 2, the prepared raw materials were placed in a crucible made of aluminum oxide, and vacuum smelting was carried out in a high-frequency vacuum induction smelting furnace in a vacuum of 5×10−2 Pa at a temperature of 1500° C. or lower.
- (2) Casting process: Ar gas was introduced into the smelting furnace after vacuum smelting to make the gas pressure reach 55,000 Pa, casting was then carried out, and a quenched alloy was obtained at a cooling rate of 102 to 104° C./sec.
- (3) Hydrogen-decrepitation-based pulverization process: A hydrogen decrepitation furnace, in which the quenched alloy was placed, was evacuated at room temperature, hydrogen with a purity of 99.9% was then introduced into the hydrogen decrepitation furnace, and the hydrogen pressure was maintained at 0.15 MPa; after full hydrogen absorption, the furnace was heated up while being evacuated, and full dehydrogenation was carried out; after cooling, a powder pulverized by hydrogen decrepitation was taken out.
- (4) Micro-pulverization process: The powder pulverized by hydrogen decrepitation was subjected to jet mill pulverization for 3 hours under the conditions of an oxidizing gas content of 100 ppm or less in a nitrogen atmosphere and a pulverization chamber pressure of 0.38 MPa to obtain a fine powder. The oxidizing gas referred to oxygen or moisture.
- (5) Zinc stearate was added to the powder resulting from jet mill pulverization in an amount as shown in Table 2, and then fully mixed by means of a V-type mixer.
- (6) Magnetic field forming process: The above-mentioned powder, to which zinc stearate had been added, was subjected to primary formation into a cube with a side length of 25 mm by means of a right-angle alignment magnetic field forming machine in a 1.6 T alignment magnetic field at a forming pressure of 0.35 ton/cm2, and after the primary formation, the powder was demagnetized in a 0.2 T magnetic field. The formed body resulting from primary formation was sealed so that it did not come into contact with air, and secondary formation was then carried out at a pressure of 1.3 ton/cm2 by means of a secondary formation machine (an isostatic pressing machine).
- (7) Sintering process: Each formed body was moved to a sintering furnace for sintering in a vacuum of 5×10−3 Pa and at temperatures of 300° C. and 600° C., each for 1 hour, and then for sintering at a temperature of 1040° C. for 2 hours, Ar gas was then introduced to make the gas pressure reach 0.1 MPa, and the formed body was then cooled to room temperature.
- (8) Grain boundary diffusion treatment process: The metal Dy or Tb and the sintered R-T-B series permanent magnet material were placed in a furnace and heated at a high temperature, such that the metal Dy or Tb was evaporated at the high temperature, deposited on the surface of the magnet under the induction of a foreign rare gas, and diffused into the interior of the magnet along the grain boundaries (specifically according to the conditions shown in Table 2).
- (9) Heat treatment process: The sintered body was heat treated for 3 hours in high-purity Ar gas at the heat treatment temperature shown in Table 2, then cooled to room temperature, and then taken out to obtain the R-T-B series permanent magnet material.
- The R-T-B series permanent magnet materials prepared in Examples 1-5 and Comparative Examples 1-7 were separately taken to measure the magnetic performance and compositions thereof, and the phase compositions of the magnets thereof were observed by means of FE-EPMA.
- (1) The compositions of the R-T-B series permanent magnet materials were measured using a high-frequency inductively coupled plasma optical emission spectrometer (ICP-OES), wherein an (RL1-yRHy)2Ti7Cx (x: 2-3, and y: 0.15-0.35) phase was obtained according to an FE-EPMA test. Table 3 below showed the composition test results.
-
TABLE 3 Composition of R-T-B series permanent magnet material and contents (wt. %) Is RL RH (RL1−yRHy)2T17Cx No. R PcNd Nd Dy Tb B C Cu Ga Ti Fe Zr Nb Co O phase generated? Example 1 30.4 / 28.5 0.6 1.3 0.93 0.12 0.12 0.12 0.16 67.27 / / 0.8 0.08 Yes Example 2 31 29 / 1.5 0.5 0.905 0.04 0.2 0.2 0.08 66.29 / / 1.2 0.09 Yes Example 3 29 / 27.5 1 0.5 0.945 0.15 0.05 0.12 0.05 68.59 / / 1 0.1 Yes Example 4 31 29.5 / 1 0.5 0.905 0.07 0.08 0.1 0.1 66.13 / / 1.5 0.12 Yes Example 5 30 / 28.5 1 0.5 0.915 0.1 0.15 0.05 0.2 66.49 / / 2 0.1 Yes Comparative 31.5 30 / 1 0.5 0.96 0.07 0.08 0.07 0.1 66.14 / / 1 0.08 Yes Example 1 Comparative 30.6 29.1 / 1 0.5 0.89 0.07 0.04 0.03 0.1 67.19 / / 1 0.08 No Example 2 Comparative 30.9 29.4 / 1 0.5 0.97 0.07 0.25 0.3 0.1 66.33 / / 1 0.08 No Example 3 Comparative 29.5 / 28 1 0.5 0.945 0.2 0.05 0.25 0.02 67.92 / / 1 0.12 No Example 4 Comparative 28.5 / 27.5 1 0.5 0.945 0.15 0.05 0.12 0.05 68.57 / / 1 0.12 No Example 5 Comparative 31 29 / 1.5 0.5 0.905 0.04 0.2 0.2 / 66.49 0.08 / 1 0.09 No Example 6 Comparative 31 29 / 1.5 0.5 0.905 0.04 0.2 0.2 / 66.49 / 0.08 1 0.09 No Example 7 Note: The above-mentioned permanent magnet materials were all prepared under the process conditions with an oxygen content of 100 ppm or less, and the difference in the O content in the final product could be regarded as a regular fluctuation; Note: “/” referred to being free of the element. - (2) FE-EPMA detection: A vertical alignment plane of the permanent magnet material was polished, and detected by means of a field emission-electron probe micro-analyser (FE-EPMA) (JEOL, 8530F). Surface scanning was firstly performed, and phases with different contrasts were then quantitatively analyzed to determine the phase composition, wherein the test conditions were an accelerating voltage of 15 kV and a probe beam current of 50 nA.
- FE-EPMA detection was carried out on the R-T-B series permanent magnet materials prepared in Examples 1-5, and the results were as shown in Table 4 below, wherein
FIG. 1 corresponded to the R-T-B series permanent magnet material prepared in Example 1 (wherein the composition ofpoint 1 was as shown in Table 4 with respect to Example 1). -
TABLE 4 R T C No. Nd Pr Tb Dy Fe Co Ga Cu Ti C Phase composition Example 1 7.11 0 0.2 1.9 76.83 1.32 0.02 0.08 0.01 12.21 (RL0.77RH0.23)2-T17-C2.7 Example 2 5.92 1.3 1.7 0.3 76.94 1.52 0..05 0.1 0.02 12.15 (RL0.78RH0.22)2-T17-C2.6 Example 3 7.06 0 1.89 0.2 76.36 1.48 0.03 0.07 0.02 12.89 (RL0.77RH0.23)2-T17-C2.8 Example 4 5.88 1.6 1.5 0.2 76.51 1.65 0.06 0.02 0.05 12.53 (RL0.81RH0.18)2-T17-C2.7 Example 5 6.58 0 2.4 0.2 76.51 1.52 0.02 0.06 0.04 12.67 (RL0.72RH0.28)2-T17-C2.8 - (3) Magnetic performance evaluation: The permanent magnet material was tested for magnetic performance by NIM-10000H BH bulk rare earth permanent magnet nondestructive measurement system from The National Institute of Metrology of China, and the magnetic performance test results were as shown in Table 5 below. In Table 5, “Br” referred to residual magnetic flux density, “Hcj” referred to intrinsic coercivity, “BHmax” referred to maximum energy product, and “BHH” referred to the sum of BHmax and Hcj.
-
TABLE 5 Performance of R-T-B series permanent magnet materials Br Hcj BHmax Heat treatment No. (kGs) (kOe) (MGOe) BHH temperature (° C.) Example 1 14.05 26.5 47.4 73.9 470-510 Example 2 13.92 28.3 46.4 74.7 460-500 Example 3 14.31 25.7 49.2 74.9 480-520 Example 4 13.98 27.1 47.0 74.1 480-520 Example 5 14.02 26.6 47.1 73.7 460-500 Comparative 13.51 26.8 43.7 70.5 480-500 Example 1 Comparative 14.03 25.8 47.1 72.9 460-470 Example 2 Comparative 13.58 27.0 44.1 71.1 480-500 Example 3 Comparative 14.28 24.1 48.9 73.0 480-490 Example 4 Comparative 14.33 17.5 49.1 66.6 480-490 Example 5 Comparative 13.88 26.4 46.1 72.5 480-500 Example 6 Comparative 13.81 26.8 45.6 72.4 480-500 Example 7 - As can be seen from Table 5,
- 1) the R-T-B series permanent magnet material of the present application has an excellent performance, maintains relatively high Br and Hcj at various heat treatment temperatures: Br≥13.92 kGs and Hcj≥25.7 kOe (Examples 1-5);
2) based on the formula of the present application, even if the contents of R, B, Cu, and Ga are adjusted, no (RL1-yRHy)2T17Cx (x: 2-3, and y: 0.15-0.35) phase can be generated, the Br and Hcj of the R-T-B series permanent magnet material cannot be both maintained at higher values, and the heat treatment temperature range is reduced significantly (Comparative Example 1 and Comparative Example 3);
3) based on the formula of the present application, even if the contents of C, Ti and Ga are adjusted, the Hcj of the R-T-B series permanent magnet material is reduced and at the same time the heat treatment temperature range will also decrease when the contents of the other compositions are not within the ranges defined in the present application (Comparative Example 4);
4) based on the formula of the present application, where the content of RH remains constant and no grain boundary diffusion is performed during preparation, no (RL1-yRHy)2T17Cx (x: 2-3, and y: 0.15-0.35) phase can be generated without introduction of RH, the Hcj significantly decreases, and the heat treatment temperature range also decreases (Comparative Example 5);
5) based on the formula of the present application, where the high melting point metal Ti is replaced with Zr and Nb respectively and the content remains unchanged, the Br and Hcj of the R-T-B series permanent magnet material decrease, and the heat treatment temperature range also decreases (Comparative Examples 6 and 7).
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